Low Resistance Microfabricated Filter

ABSTRACT

The present technology provides micro fabricated filtration devices, methods of making such devices, and uses for microfabricated filtration devices. The devices may allow diffusion to occur between two fluids with improved transport resistance characteristics as compared to conventional filtration devices. The devices may include a compound structure that includes a porous membrane overlying a support structure. The support structure may define a cavity and a plurality of recesses formed in a way that can allow modified convective flow of a first fluid to provide improved diffusive transport between the first fluid and a second fluid through the membrane.

TECHNICAL FIELD

The present technology relates to filtration devices and methods ofmaking and using filtration devices. More specifically, the presenttechnology relates to making and using microfabricated filters.

BACKGROUND

Filtration devices are used in a variety of ways to provide purifiedmaterials. As technology improves, sensitive processes may requirehighly purified materials to be provided, and thus improved filters maybe required. Micro and nanofabrication may be used to produce fine meshfilters for use in such processes. However, as filter dimensioningdecreases, manufacturing issues such as brittleness and performanceissues such as breakdown may increase. Additionally, as filter poredimensions decrease, pressure gradients may increase above useablethresholds. Accordingly, there is a need for improved filtration devicesand methods of making such devices. These and other needs are addressedby the present technology.

SUMMARY

Microfabricated filters according to the present technology may includea planar membrane section including a plurality of pores. Each pore ofthe plurality of pores may have a width of less than or about 100 nm.The devices may further include a support section including a substratecoupled with the membrane section. The substrate may include a pluralityof thick portions and a plurality of recesses between the thick portionsand a second thin portion that is between adjacent thick portions. Therecesses may be in communication with the pores in the plurality ofpores. The thin portion of the substrate may be characterized by athickness of between about 10 μm and about 100 μm. The thin portion mayalso be characterized by thicknesses of between about 20 μm and about 50μm. The microfabricated filtration device may further include anadditional layer of material between the substrate and the membranesection. In disclosed embodiments, the additional layer of material mayinclude a dielectric material.

Methods of using microfabricated filtration devices are also described.The methods may include delivering the fluid to a filtration device, andthe filtration device may include a planar membrane section including aplurality of pores. Each pore of the plurality of pores may have a widthof less than or about 100 nm. The device may further include a supportsection including a substrate coupled with the membrane section. Thesubstrate may include a plurality of thick portions and a plurality ofrecesses between the thick portions and a second thin portion that isbetween adjacent thick portions. The recesses may be in communicationwith the pores in the plurality of pores. The methods may furtherinclude flowing the fluid over the planar membrane section to produce afiltered fluid. The methods may still further include delivering thefiltered fluid from the filtration device. The filtration device mayfurther include a first channel in fluid communication with the membranesection of the filtration device, and a second channel in fluidcommunication with the support section of the filtration device. Themethods may further include flowing the first fluid through the firstchannel in a first direction of flow. The methods may also includeflowing a second fluid through the second channel in a direction of flowthat is countercurrent to the first direction of flow. The methods mayfurther include transporting solutes across the membrane section betweenthe first fluid and the second fluid. The methods may still furtherinclude pumping the first and second fluid through the filtration deviceto maintain equal pressure across the membrane section of the filtrationdevice. The methods may also include incorporating an additionalmaterial into the first fluid prior to delivering the fluid to thefiltration device.

The disclosed technology further encompasses microfabricated filtrationdevices having a membrane section having a thickness of less than about1 μm in height, and defining a plurality of pores having a width of lessthan about 10 nm. The filtration devices may further include a supportsection including a substrate coupled with the membrane section, wherethe substrate at least partially defines a cavity and a plurality ofrecesses. The cavity may be located within the backside of the substrateand may be in communication with the plurality of recesses, where therecesses are in communication with the defined pores. Additionally, theplurality of recesses may be defined by portions of the substrate suchthat each portion of the substrate located between any two recessescomprises a height of about 50 μm or less. The support section of thefiltration devices may further include at least one additional layer ofmaterial disposed between the substrate and membrane sections, where theat least one additional layer may define a portion of the recesses. Theportions of the substrate located between any two recesses may becharacterized by a height of about 20 μm or more. The plurality ofrecesses may be characterized by a diameter of less than about 150 μm.The substrate of the microfabricated filtration device may becharacterized by a single homogenous layer of material. The cavitydefined in the microfabricated filtration device may include inwardlysloping walls toward the plurality of recesses. The plurality ofrecesses within the microfabricated filtration device may becharacterized by length by width measurements of about 100 μm by about50 μm.

Additional methods of making microfabricated filtration devices are alsodisclosed. The methods may include depositing a dielectric layer over asemiconductor substrate. The methods may additionally include forming afirst layer of a membrane material on the dielectric layer and etching apattern in the first membrane material layer. The methods may alsoinclude forming a sacrificial dielectric layer over the patterned firstmembrane material layer, and forming a second membrane material layerover the sacrificial dielectric layer. The methods may also includeforming a protective layer over the second membrane material layer. Themethods may further include etching the substrate with a first etchantprocess that produces a cavity that does not extend to the layers ofmembrane material. The methods may also include etching the substratewith a second etchant process that forms a plurality of recesses throughthe remaining portion of the substrate. The methods may also includeetching the filtration device with a third etchant process that removesthe sacrificial dielectric layer forming pores through the membranematerial layers, which provides access to the recesses such that thecombination of the pores, recesses, and the cavity produce aperturesthrough the filtration device. The first etching process may include awet etchant in disclosed embodiments, and in disclosed embodiments thefirst etchant process and the second etchant process may include areactive ion etch.

Additional methods of filtering fluid are also encompassed by thetechnology, and may include delivering a first fluid into a filtrationdevice. The methods may further include flowing the first fluid acrossthe front side of a filtration member located in the filtration devicethat includes a membrane section having a thickness of less than about 1μm in height, and defining a plurality of pores having a width of lessthan about 10 nm. The methods may also include flowing a second fluidacross the backside of the filtration member located in the filtrationdevice that includes a support section comprising a substrate coupledwith the membrane section, with the substrate at least partiallydefining a cavity and a plurality of recesses. The cavity may be locatedin the backside of the substrate and may be in communication with theplurality of recesses, where the recesses are in communication with thedefined pores. The plurality of recesses may be defined by portions ofthe substrate such that each portion of the substrate located betweenany two recesses may be characterized by a height of about 50 μm orless. The second fluid may flow through the cavity to provide the secondfluid to the recesses such that solute transport may occur across themembrane section between the first and second fluids to produce filteredfirst fluid. The methods may further include transferring the filteredfirst fluid from the filtration device.

Such technology may provide numerous benefits over conventionaltechniques. For example, improved filtration may be provided based onthe reduced thickness of the filtration pores produced in the discloseddevices. Additionally, reduced manufacturing queue times may be affordedby the fabrication processes described. These and other embodiments,along with many of their advantages and features, are described in moredetail in conjunction with the below description and attached figures.

BRIEF DESCRIPTION OF THE DRAWINGS

An understanding of the nature and advantages of the disclosedtechnology may be realized by reference to the specification anddrawings.

FIG. 1 shows a cross-sectional view of a filter fabricated according toembodiments of the present technology.

FIG. 2A shows a top view of an array of membranes as may be disposed ona support structure according to embodiments of the present technology.

FIG. 2B shows a cross-sectional view along lines A-A of FIG. 2A of afilter fabricated according to embodiments of the present technology.

FIGS. 3A-3F show cross-sectional views of a filter during certain stepsof a method for making a filter according to embodiments of the presenttechnology.

FIG. 4 shows an exemplary use of a filter according to embodiments ofthe present technology for allowing diffusive transport between twofluids.

FIG. 5 shows a flow chart of a method of fabricating a filter accordingto embodiments of the present technology.

FIG. 6 shows a flow chart of a method of using a filter according toembodiments of the present technology.

FIG. 7 shows a graph of the diffusion resistance associated with afilter structure.

FIG. 8 shows a graph of the modeled flow of a fluid along the backsideof a filter fabricated according to embodiments of the presenttechnology.

FIGS. 9A-9C show cross-sectional views of a filter during certain stepsof a method for making a filter according to embodiments of the presenttechnology.

FIGS. 10A-10C show cross-sectional views of a filter during certainsteps of a method for making a filter according to embodiments of thepresent technology.

FIGS. 11A-11C show cross-sectional views of a filter during certainsteps of a method for making a filter according to embodiments of thepresent technology.

FIGS. 12A-12C show cross-sectional views of a filter during certainsteps of a method for making a filter according to embodiments of thepresent technology.

FIG. 12D shows SEM images of exemplary structures produced according toembodiments of the present technology.

FIGS. 13A-13D show cross-sectional views of a filter during certainsteps of a method for making a filter according to embodiments of thepresent technology.

FIGS. 14A-14D show cross-sectional views of a filter during certainsteps of a method for making a filter according to embodiments of thepresent technology.

FIGS. 15A-15D show cross-sectional views of a filter during certainsteps of a method for making a filter according to embodiments of thepresent technology.

FIG. 16 shows SEM images of exemplary structures produced according toembodiments of the present technology.

In the appended figures, similar components and/or features may have thesame numerical reference label. Further, various components of the sametype may be distinguished by following the reference label by a letterthat distinguishes among the similar components and/or features. If onlythe first numerical reference label is used in the specification, thedescription is applicable to any one of the similar components and/orfeatures having the same first numerical reference label irrespective ofthe letter suffix.

DETAILED DESCRIPTION

The present technology provides microfabricated filtration devices,methods of making such devices, and uses for microfabricated filtrationdevices. In one example, the filtration devices may allow diffusion tooccur between two fluids with improved transport resistancecharacteristics as compared to conventional filtration devices. Thedevices may include a compound structure that includes a membraneoverlying a support structure. The support structure may define a cavityand a plurality of recesses formed in a way that can allow modifiedconvective flow of a first fluid to provide improved diffusive transportbetween the first fluid and a second fluid through the membrane.

FIG. 1 shows a cross-sectional view of a microfabricated filter 100fabricated according to embodiments of the present technology. Thefilter 100 includes a membrane section 115 overlying a substrate section105. The filter may include one or more additional layers 110 betweenthe membrane section 115 and substrate section 105 in variousconfigurations. For example, an additional layer 110 may be includedthat acts as an etch stop layer during fabrication, a protectivecoating, a structural member to provide extra rigidity or flexibility,etc. The additional layers may be of the same or a different material asthe membrane or substrate layers.

The substrate section 105, which may act as a support section for themembrane 115, may be a silicon wafer as is conventionally used inmicrofabrication, and may be, for example, a silicon wafer that may havea variety of crystal orientations including a [100] plane orientation aslisted by the Miller indices. The substrate may be a 100 mm diametersilicon wafer having a thickness of 400 μm, but can also be larger orsmaller diameters including about 76 mm or smaller, or about 150 mm,about 200 mm, about 300 mm, about 450 mm, etc., or larger. Additionally,the thickness of the wafer may be based on convention for the diameterof the wafer, but may also be less then about 400 μm, about 600 μm,about 700 μm, about 900 μm, etc. or more. The substrate may additionallybe germanium, Group IV elements of the periodic table, III-V compoundsincluding gallium arsenide, II-IV compounds including zinc tellurium, pand n doped compounds, etc.

The membrane section 100 may be formed with any number of materials thatcan be deposited or grown on a micro- or nano-thick scale on a substrate105 or intermediate layer 110. For example, the membrane material may bemade with silicon, polysilicon, silicon carbide, ultrananocrystallinediamond, diamond-like-carbon, silicon dioxide, PMMA, SU-8, PTFE,titanium, silica, silicon nitride, polytetrafluorethylene,polymethylmethacrylate, polystyrene, silicone, or various othermaterials. The additional layer or layers 110 may include a dielectricmaterial such as a nitride or oxide layer, including silicon nitride forexample, as well as flexible materials including elastomers or materialsproviding strength and/or rigidity to the filter structure, includingmetals, ceramics, and polymers.

Among the final stages of fabrication may include the production orformation of pores 120, which may be produced by the removal of asacrificial material, for example, from the membrane section 115, whichmay include a planar membrane. The pores may be of various shapesincluding linear, square, circular, ovoid, elliptical, or other shapes.In some embodiments, the plurality of nanofabricated pores have a widthless than 100 nm, e.g., less than or about 50 nm, 20 nm, 15 nm, 10 nm, 7nm, 5 nm, 3 nm, etc., or less. In some embodiments, the distance, e.g.,average distance, between each of the plurality of nanofabricated poresmay be less than about 500 nm, and may be less than or about 50 nm, 100nm, 150 nm, 200 nm, 250 nm, etc., or more. In some embodiments, thelength of the nanofabricated pores may be less than about 200 μm, andmay be less than 100 μm, 50 μm, 40 μm, 30 μm, 10 μm, etc., or less. Insome embodiments, the plurality of nanofabricated pores have a slitshape. In some embodiments, the membrane 115 comprises more than onepore, where the pores comprise a single shape or any combination ofshapes. In some embodiments, a membrane comprises more than one pore,where the pore sizes range from about 10 to about 100 μm in anydimension; the dimensions need not be the same in any particular poreshape, and the pores may comprise a single size or any combination ofsizes. Additionally, the pores may be lined up from membrane tomembrane, or offset from one another in various fashion across or withinmembranes. The pore size formed may be dictated by the process for whichthe filtration device may be utilized. For example, if the device isused for diffusion in a dialysis process, the pores may be able to allowfor diffusion of ions and nutrients, but may substantially prevent theflow of albumin and cellular material through the membrane.

During the fabrication of the filters, apertures may be formed that mayinclude the pores 120, as well as a plurality of recesses 130 that arein communication with the pores, and one or more cavities 125. Theapertures may be formed to provide access to the membrane structure fromthe backside of the filter, i.e., through the substrate 105, and may beformed to produce an array of functioning membranes 115 as will bedescribed in more detail below. The apertures may include a cavity 125through which a fluid may be transported. The cavity 125 provides accessto a plurality of recesses 130 that are separated by divisions 135 thatmay be formed by portions of the substrate 105, and may be thin portionsof the substrate as compared to the thicker support sections definingthe lower parts of the cavity, as well as any intermediate or additionallayers 110 that are located above the substrate 105. The substrate mayinclude a thicker portion located nearer the backside of the substrate,as well as a thinner portion located nearer the front side of thesubstrate. The thicker portion may define the cavity 125 across thesubstrate, while the thinner portion may define the plurality ofrecesses 130 located between the thick portion defining the cavity 125and the membrane 115. When a fluid is flowed through the cavity 125, thefiltration device may allow for diffusive transport across the membranesection 115 through the pores 115 and recesses 130. The cavity 125 mayhave walls that slope towards the diffusive recesses as shown in theFigure. Such sloping may provide improved flow characteristics, byproviding a more streamlined flow of a fluid forced across thestructure, although in other embodiments the structure may have moresquare walls or shapes. By providing the cavity, several benefits may beprovided including reducing the resistance through the diffusiverecesses, and being able to provide a refreshed fluid more often acrossthe recesses. For example, the filtration device may be used during afluid filtration process including hemodialysis that may involvediffusion and/or ultrafiltration. By reducing the diffusive resistance,less membrane surface may be needed as will be explained below.Additionally, by improving the flow of fluid across the substrate, therefresh rate of the fluid being used may be improved.

FIG. 2A shows a top view of an array 200 of membranes 205 as may bedisposed on a support structure according to embodiments of the presenttechnology. The array may include various configurations of membranes205 separated by dividers 210. The dividers 210 may provide severalbenefits including anchoring the pores located across the membranes, aswell as providing structural support to the membrane 205 as a whole. Themembrane structures 205 may be patterned over an area of a substratethat may include lengths as small as several microns, or as large asseveral millimeters. In some embodiments, the entire surface of thesubstrate may be patterned with the membrane structure, whilealternatively less than the entire surface may be patterned to improveuniformity in thickness or configuration, for example.

FIG. 2B shows a cross-sectional view along lines A-A of FIG. 2A of afilter fabricated according to embodiments of the present technology.This sectional view is not necessarily to scale, nor as wouldnecessarily be located along the periphery of a substrate. In someembodiments a greater or fewer number of layers may be incorporated, forexample, including an etch stop layer. This view is intended to aid oneof skill in conceptualizing the structure of an embodiment of thefiltration device without limiting the scope of the technology disclosedherein. The cross-section shows the location of apertures 215 formedthrough the membrane sections 205. In practice, the apertures may beformed in a pattern or array on the underside of the substrate toprovide access through the membrane surface. The apertures 215 may be ofany shape or size, and may be formed at particular intervals along thesubstrate to produce useable membranes at specific locations to providea determined area of filtration across the device. The apertures may beformed as sections including one or more pores through the membrane, adiffusive recess, and a cavity. Exemplary recesses may have a diameterof less than or about 500 μm, with diameter referring to a straight linepassing from side to side of any figure regardless of actual shape. Forexample, a rectangular recess may be formed with lengths less than 500μm each. Recesses may be of any shape or dimensions, including square,rectangular, circular, elliptical, etc., or other geometric figures, andmay reach to the limits of the substrate dimensions. Exemplary recessesmay be rectangular, and may comprise side lengths less than or about 400μm, 300 μm, 200 μm, 100 μm, 75 μm, 60 μm, 50 μm, 40 μm, 30 μm, 20 μm, 10μm, etc. or less. In one embodiment the recesses are rectangular andhave length by width dimensions of about 120 μm by 60 μm. Alternativerecesses may have dimensions of 100 μm by 50 μm, or less, and mayinclude other combinations as would be understood by one of skill. Thedimensions of a recess may depend on several variables including thepressure that may be applied to or across the membrane, the materialused for the membrane section, etc. Recesses formed in filtrationdevices according to embodiments of the present technology may besmaller than can some conventional recesses due to the increasedpermeability that may be produced by the structure of the device. Thisfeature will be explained in still greater detail below.

The exemplary support structure 210 as can be seen in thecross-sectional view does not show the cavity located below theremaining support structures 210 formed across the structure andproviding access to the diffusive recesses 230. The recesses 230 may beseparated by dividers 235 that include portions of the substrate. Thedividers 235 provide structural support to the membrane 205, while alsodefining the diffusive recesses 230 through which transportation canoccur. As can be appreciated by the view of FIG. 2, although the entiresurface of the filtration device may be structured with the membranesection 205, the functional portions of the membrane may be defined bythe areas under which the recesses are formed. The process of formingrecesses under the membranes provides the paths or apertures throughwhich transportation can occur. The process for forming apertures willbe described below with reference to FIGS. 3A-3F.

FIGS. 3A-3F show cross-sectional views of a filter during certain stepsof a method for making a filter according to embodiments of the presenttechnology. As described previously, and shown in FIG. 3A, a substrate305 may be provided on which the membranes are formed. In one example,the substrate is a silicon substrate having a diameter of about 100 mmand a thickness of about 400 μm, although substrates of differingmaterials and dimensions can be used to equivalent effect. A protectiveoxide or nitride layer 310 may be deposited over the substrate. Thelayer 310 may include a silicon nitride, silicon oxide, siliconoxynitride, silicon carbide, or some other layer of material includingother dielectric materials and combinations. For example, multiplelayers of oxide, a combined layer of oxide and nitride, etc., may formlayer 310. Additionally, multiple layers may be grown or deposited incombination for layer 310. The thickness of the protective layer 310 maybe about 5 μm in one example.

Alternatively, the protective layer may be less than or about 10 μm, 7μm, 4 μm, 3 μm, 2 μm, 1 μm, 500 nm, 400 nm, 300 nm, 200 nm, 100 nm, 50nm, 10 nm, etc., or less. The protective layer 310 may be deposited byCVD including LPCVD and PECVD, or by some other deposition means. Forexample, the protective layer may be grown with a thermal process. Ontothis protective layer may be deposited a first membrane material layer315 such as polysilicon, in one example. The first membrane material maybe deposited by the same or a different deposition means, and mayinclude LPCVD in one example. The thickness of the first membranematerial layer may be about 5 μm in one example. Alternatively, thefirst membrane material layer 315 may be less than or about 10 μm, 7 μm,4 μm, 3 μm, 2 μm, 1 μm, 750 nm, 500 nm, 450 nm, 400 nm, 350 nm, 300 nm,250 nm, 200 nm, 150 nm, 100 nm, 50 nm, 25 nm, 10 nm, etc., or less. Instill another embodiment, the substrate used may be asilicon-on-insulator (SOI) and a protective layer may not beadditionally deposited over the existing material of the substrate.

FIG. 3B shows the formation of a pore structure in the membrane materiallayer. The pore structure may be formed with a sacrificial material thatmay be later removed to form pores through the membrane material. Thepore structure 320 may be formed with an etching process, or otherlithography process. The first membrane material layer 315 may bepatterned with a photoresist that may be performed via e-beam, deepultraviolet lithography, or another patterning technique that can formpatterning for creating structures as described herein. The resistpattern may be transferred via a reactive ion etch or wet etch processonto the first membrane material layer 315. Following the patterning, asacrificial layer of material may be formed on or within the patternedfirst membrane material layer 315. The sacrificial layer may be an oxidegrown via thermal oxidation that may be less than 20 nm thick.Alternatively, the layer may have a thickness of less than or about 15nm, 10 nm, 7 nm, 5 nm, 3 nm, 1 nm, 5 angstrom, etc., or less. The layerof material may be conformal when grown, and thus the film may be formedvia a more conformal process including HDPCVD, or some other conformaldeposition process. The layer may be silicon oxide, or any othermaterial that can be subsequently removed from the membrane section tocreate the pores.

The layer of sacrificial material may be selectively removed in certainareas with a subsequent photoresist patterning and etch. This mayprovide areas for anchoring a second membrane material layer to thefirst membrane material layer during a subsequent deposition. Afterremoving the photoresist, a second membrane material may be depositedfilling in the anchor cavities, as well as the areas around thesacrificial layer in and around the trenches formed in the firstmembrane material. This material may be the same or a different membranematerial as previously described. For example, the second membranematerial may also be polysilicon. The second membrane material layer maybe about 5 μm in one example. Alternatively, the protective layer may beless than or about 4 μm, 3 μm, 2 μm, 1 μm, 750 nm, 600 nm, 500 nm, 400nm, 300 nm, 200 nm, 100 nm, 50 nm, 10 nm, etc., or less. The secondmembrane material layer may be planarized down at least to a levelexposing the sacrificial material, and thereby forming the porestructure 320. The planarization may occur with any polishing or etchingtechnique, and can include a reactive ion etch in one example. In stillanother example, the anchors may be formed and filled subsequent todepositing the second membrane material and performing a planarization.The process may alternatively be performed by performing an additionallithography step followed by a direct etching, such as with a reactiveion etch, followed by a specific deposition for the anchor material.

The pores may also be more densely patterned by performing a series ofpatterning and deposition processes. For example, subsequent to theinitial deposition of the membrane material, a secondary patterning stepsimilar to that as described above may be performed. Once the secondarypatterning has been performed, an additional protective layer may bedeposited in a way as previously described. Following the formation ofthe additional protective layer, a subsequent layer of membrane materialmay be formed to provide the degree of pore spacing required. Therepetitive processing may reduce the line and space pattern by 20% ormore. Alternatively, the repetitive processing can reduce the line andspace pattern by about 30% or more, about 40%, about 50%, about 55%,about 60%, about 65%, about 70%, about 75%, about 80%, about 85%, about90%, etc., or more. In one example, by performing a subsequent series ofpatterning and formation, an initial patterning process of 450 nmline/space pattern can be reduced to 150 nm or less. By maintaining theprotective material within the pores during fabrication, pore integritymay be maintained until a final release is performed.

FIG. 3C shows that a second protective layer 322 is applied over themembrane materials 315 prior to the backside processes. The secondprotective layer may include an oxide, nitride, or another compounddepending on the etching technique subsequently performed. For example,a nitride layer may be deposited if a potassium hydroxide etch isperformed, and an oxide layer may be deposited if the subsequent etchincludes a chemical selective to nitrogen, such as tetramethylammoniumhydroxide.

FIG. 3D shows a first etchant process that can be performed on thebackside of the filtration device. A cavity 325 may be etched throughthe substrate 305 that may not remove material to the level of the firstprotective layer 310. The first etchant may be a wet etchant, that maybe, for example, potassium hydroxide, tetramethylammonium, bufferedhydrofluoric acid, EDP, etc. The determination of when to stop the etchprocess can be based on a desired thickness of remaining substrate. Thefirst wet etch may be isotropic or orientation selective, i.e.,anisotropic. As shown in FIG. 3D, in an exemplary first etch process,KOH is used to produce sloped sides of the substrate 305 for theconvective cavity. Because certain etchants including KOH, EDP, and TMAHdisplay an etch rate selective to [100] orientation over [111]orientations, sloped walls can be produced defining the convectivecavity. In other embodiments, etchants can be used that are moreanisotropic and produce little or no sloping of the cavity walls.Additionally, a reactive ion etch may be performed for the first etchantprocess. Additionally, multiple cavities can be formed across the bottomof the substrate. In some examples, cavities are etched asymmetricallyacross the substrate. A plurality of cavities etched may have the sameor different dimensions. In one example, relatively square cavities maybe etched that may be about 1 mm per side or more. Alternatively thecavities may be about 2 mm per side, about 3 mm, about 5 mm, about 7 mm,about 10 mm, about 12 mm, about 15 mm, about 17 mm, about 20 mm, etc.,or more. Alternative geometries having any of the dimensions per side asdescribed herein can also be etched as cavities in the substrate.

Following the formation of the cavity 325, patterning can be formed onthe backside of the substrate in order to form the desired recesses 330as illustrated in FIG. 3E. The patterning can be formed on the remainingexposed substrate at the top portion of the cavity 325. The patterningcan create windows of any of the shapes and dimensions as previouslydescribed through which the etching of the recesses may be performed.For example, windows of 100 μm by 50 μm may be formed in variouspatterns across the bottom of the substrate for the formation ofdiffusive recesses. In an alternative example, the windows may be 250 μmby 50 μm. Depending on the size of the substrate, many such windows canbe formed depending on the dimensions and the width of material leftbetween the windows. For example, on a 100 mm diameter substrate, morethan 20,000 windows or more could be patterned that are roughly 100 μmby 50 μm. A certain amount of substrate may be provided between eachwindow in order to provide structural support for the membrane whenexposed. The amount of substrate left between each window may be lessthan or about 100 μm on each side. Alternatively, the amount ofsubstrate left between each window may be less than or about 80 μm, 70μm, 60 μm, 50 μm, 40 μm, 35 μm, 30 μm, 25 μm, 20 μm, 17 μm, 15 μm, 12μm, 10 μm, 7 μm, 5 μm, 3 μm, 1 μm, 500 nm, etc., or less. The windowsmay also be formed in other patterns based on the dimensions of thecavity formed. For example, if a cavity is etched by the processdescribed within a 10 mm square area, and the windows have dimensions ofabout 250 μm by 50 μm, for example. The area may provide fewer than 1000windows in one example. Alternatively, the area may provide more thanabout 1000 windows, about 1200, about 1300, about 1500, about 1700,about 2000, about 2300, about 2500, about 2700, about 3000, about 3500,etc. or more.

The etching to form the diffusive recesses may be a dry etch process,and may include reactive ion etching or a Bosch or other deep etchingprocess. The etching may be performed to the level of the firstprotective layer 310 originally deposited over the substrate 305surface, thereby using the material as an etch stop layer. After theetching is complete, the height of the diffusive recesses may be lessthan about 100 μm. Alternatively, the height of the diffusive recessesmay be less than or about 90 μm, 85 μm, 80 μm, 75 μm, 70 μm, 65 μm, 60μm, 55 μm, 50 μm, 45 μm, 40 μm, 35 μm, 30 μm, 25 μm, 20 μm, etc., orless. Alternatively still, the height of the diffusive recesses may begreater than or about 1 μm, 2 μm, 3 μm, 5 μm, 10 μm, 15 μm, 20 μm, 25μm, 30 μm, 35 μm, 40 μm, 45 μm, 50 μm, 55 μm, 60 μm, etc., or greater.In still another alternative, the height of the diffusive recesses maybe between about 0 μm and 400 μm, 0 μm and 300 μm, 0 μm and 200 μm, 0 μmand 100 μm, 10 μm and 80 μm, 10 μm and 60 μm, 20 μm and 60 μm, 20 μm and50 μm, 30 μm and 50 μm, etc. By maintaining the height of the diffusiverecesses 330 greater than about 20 μm or more, improved structuralintegrity may be produced that may affect membrane integrity during bothfabrication and utilization of the filtration device membranes.

FIG. 3F shows an exemplary resultant filter after a third etch processis performed. After the diffusive recesses have been formed, mechanicalprocesses including chip dicing may be performed. The diced chips may beof any dimension, and may be based on the dimension of the cavitiesformed in the substrate and the amount of space between successivecavities. For example, each chip may be 10 mm square. This dimensionedchip includes a cavity of less than 10 mm square, and a plurality ofwindows. The sized substrates may then be etched with a third etchant toremove the second protective layer 322, as well as the portions of thefirst protective layer 310 that have been exposed as a result of thesecond etch process forming the recesses. Additionally, the thirdetchant may include multiple etchants optimized for the particularmaterials sought to be removed. For example, if both a nitride and oxidelayer are sought to be removed, a phosphoric acid wash followed by ahydrofluoric acid wash may be performed. Once these layers have beenremoved, the third etchant may also remove the sacrificial material ofthe pore structures 320 in order to expose the pores 327, which completethe apertures. The resultant filtration devices may then be utilized forfiltration purposes. The third etchant may be, for example a wetetchant, and may be an etchant capable of dissolving each of theprotective layers and sacrificial layers. In one example, a hydrofluoricacid may be used.

After the chips are diced and the pores are exposed, filters may bedeveloped with one or more membrane chips. For example, a filter may becomposed of a single chip. Alternatively, a number of chips may becombined in various ways to produce a filter with a greater surface areaof membrane available. Chips may be combined laterally or vertically invarious formations. In one example, a series of chips may be stacked inalternately opposing formation to produce channels between twomembranes. A series of parallel channels may be formed in this way, anda filter may be composed of a plurality of these channels. The spacingof a channel may be defined by the spacing between the two membranes. Inone embodiment, the spacing may be about 1000 μm between two membranesforming a channel of equivalent width. Alternatively, the channel formedmay be greater than 1000 μm in width. In still alternative examples, thespacing may be less than about 1000 μm in width, and may be less thanabout 800 μm, about 600 μm, 500 μm, 400 μm, 300 μm, 250 μm, 200 μm, 150μm, 100 μm, 50 μm, 10 μm, 1 μm, 800 nm, 600 nm, 500 nm, 400 nm, 300 nm,250 nm, 200 nm, 150 nm, 100 nm, 50 nm, etc., or less.

The number of chips stacked laterally, and the number of channelscreated vertically may vary depending on the amount of active membranesurface area required for a specific filter. For example, filters may beformed that have more or less effective surface area based on the numberof chips included in the filter. The number of chips used in the filtermay be determined by the required dimensions of the filter, or by therequired effective surface area of the filter. In one exemplary filter,channels having a length of a single chip are formed. The channels mayinclude alternately opposing orientations such that every two membranesare directed towards each other, and the interposing chips are directedwith the membranes away from each other, i.e., the backside of the chipsface each other. For example, a filter having two such primary channelsmay include four chips. A primary channel for a first fluid may beformed by the spacing between the membrane side of the chips, and asecondary channel for a second fluid may be formed by the spacingbetween the backside of two chips. With an exemplary four chips, twoprimary channels divided by one secondary channel may be formed. Otherfilters may include more or less than 3, 4, 5, 6, 7, 8, 9, 10, 12, 14,16, 18, 20, 50, 75, 100, 150, 200, etc. or more channels. Additionally,the number of chips may be based on the required surface area forfiltration. For example, if roughly 0.1 square meters of filtrationmembrane area is required, this can be developed from a few or severaldozen chips organized laterally and/or vertically. Alternatively, thesame effective surface area of membrane material can be presented bylaterally increasing the number of chips. For example, a primary channelcan be created with four chips, with two chips laterally disposed andfacing another two chips laterally disposed. Many other combinations ofchips/channels can be formed, and one of skill can appreciate that avirtually limitless set of channel/chip combinations can be made todevelop filters of almost any size, shape, effective membrane surfacearea, or number of channels based on the above description.

FIG. 4 shows one exemplary filtration use, and displays a use of afilter according to embodiments of the present technology for allowingdiffusive transport between two fluids. The filtration device 400utilizes a filtration member formed, for example, as previouslydescribed for filtration of a fluid utilizing a second fluid. Oneexemplary case includes hemodialysis. In such a process, a first fluid450, which may be blood or plasma, flows across the membrane section 415of the filtration member. A second fluid 460, which may be dialysate,flows below the filtration member, and may flow up through the cavity425 defined by the substrate 405. The fluids may flow in a countercurrent fashion, but may also flow concurrently. One or both fluids mayhave additional materials incorporated into the flow, such as, forexample, an anticoagulant including heparin incorporated with the firstfluid 450. The fluids may flow naturally or be pumped through thechannels with additional pumping mechanisms (not shown). As the twofluids flow, they may be flowed with or without a pressure gradientbetween the fluids. For example, the hydrostatic pressure of the secondfluid 460 may be reduced in order to provide ultrafiltration, or freewater removal, from the first fluid 450. The filtration device 400 maybe extracorporeal or be biocompatible for in vivo use. The filtrationdevice may additionally include sensors (not shown) for determiningpressure, flow, temperature, concentration of various compounds, etc. Asthe fluids flow across the filtration member, a concentration gradientmay exist to diffuse solutes across the membrane 415 and through thepores 420 and diffusive recesses 430 in either direction. Such aconcentration gradient may allow for the first fluid to release wastes,or receive nutrients from the second fluid. The second fluid 460 mayflow up into the substrate 405 into the cavity 425, which may reduce thedistance through which diffusion must occur, and may additionallyrefresh the second fluid 460 more readily in that region. After thediffusive exchange has occurred, the first fluid may be transferred backto its originating location, such as to a patient, as a filtered fluid.

FIG. 5 shows a flow chart of a method 500 of fabricating a filteraccording to embodiments of the present technology. The method mayinclude depositing 510 a dielectric layer over a substrate to produce anetch stop layer during thinning. The dielectric layer may be an oxide,nitride, or some other material that may protect the substrate fromdownward processes, and/or materials deposited over the dielectric layerfrom upward processes. Over the dielectric layer may be formed 515 afirst membrane material layer that will become at least a part of aporous membrane. The first membrane material may be silicon based,including polysilicon, or may be some other material including metals,ceramics, and polymers chosen for qualities that may include theirrelative flexibility or rigidness.

The first membrane material may be etched 520 via a reactive ion etch orsome other etching process that may involve a lithographic patterningprocess in order to form a pattern with which a pore structure may bedeveloped. A sacrificial dielectric layer may be formed 525 over thepatterned first membrane material to create the pore structures as willbe later formed. The sacrificial layer may be an oxide or nitride orother material that is thermally grown over the first membrane material.The sacrificial layer may alternatively be grown by some otherdeposition method that can produce substantially conformal films ofminimal thickness that may be, for example, about 10 nm, 7 nm, 5 nm, 3nm, 1 nm, etc., or less. A second membrane material may be formed 530over the first membrane material and sacrificial dielectric layer. Thesecond membrane material may be of a similar or different material thanthe first membrane material, and may be, in one example, polysilicon, orsome other metal, ceramic, or polymer material. The second membranematerial may additionally be chosen based on particular properties orcharacteristics including the relative flexability, rigidness, corrosionresistance, etc., of the material.

A protective layer may be formed 535 over the membrane materials priorto etching or further processing of the filtration device. Theprotective layer may be selected to be resistant to an etchant that maybe used in subsequent processing steps, and may be an oxide, nitride, orsome other material that may resist removal during a subsequent etchingprocess. The filtration device may be etched 540 with a first etchant toproduce one or more cavities from the backside of the substrate. In oneembodiment a single cavity may be formed across the entirety of thesubstrate. The cavity may be formed to extend only partially through thesubstrate, and may not reach the level of the protective dielectricmaterial initially deposited over the substrate. The cavity may extendthrough a certain percentage of the distance of the substrate that isless than about 100%, and may be less than about 99%, 98%, 97%, 96%,95%, 94%, 93%, 92%, 91%, 90%, 85%, 80%, 75%, 70%, 65%, 60%, 55%, 50%,45%, 40%, etc., or less. Alternatively, the protective layer mayadditionally be selectively patterned on the backside of the substratein order to allow the formation of more than one cavity that areseparated by the portions of the substrate remaining under theprotective layer. The first etchant may be a wet or dry etchant, and inone example is a wet etchant that may be KOH or TMAH, and in anotherembodiment is a dry etchant comprising a reactive ion etch.

A second etching may be performed 545 to define recesses through theremaining substrate material. The second etching may be performedthrough the entire remaining substrate, and to the layer of thedielectric material previously formed over the substrate. The secondetching may include a previous patterning to define windows throughwhich the second etching may be performed. The windows may be of variousgeometries, and the resultant recesses may provide access to themembrane layers. The second etching may be a wet or dry etch, and may bea substantially anisotropic etch performed by a reactive ion etch,including a deep reactive ion etch process that extends to or past thelevel of the dielectric layer deposited over the substrate.

A third etching may be performed 550 to remove the protective layer andthe exposed dielectric layer. The etching may also remove thesacrificial layer of material thereby exposing the pores through themembrane material layers. The third etching may be a wet or dry etching,and in one example may be a hydrofluoric acid etch. After the pores havebeen exposed, a plurality of apertures may exist that include at leastone pore, the associated diffusive recess, and the cavity formed throughthe first, second, and third etching processes.

FIG. 6 shows a flow chart of a method 600 of using a filter according toembodiments of the present technology. The method may include delivering610 a first fluid to a filtration device. The filtration device mayinclude channels for a first and second fluid, as well as a filtrationmember that can allow filtering of the fluids in the channels. The firstfluid may be directed, flowed, or pumped 615 across a front side of thefiltration member that may have a membrane with a number of pores formedtherein. The pores may be of any shape and size, and may be slices orslits formed through the membrane section. A second fluid may be flowed620 across the backside of the filtration member, and may be capable offlowing into a cavity formed in the backside of the filtration membersupport structure and across a plurality of recesses that provide accessto the membrane section and pores. As the first and second fluid flowacross the filtration member, diffusive transport may occur between thefluids in either or both directions. The transport may be based on aconcentration gradient of solutes between the fluids. The fluids mayhave a net zero pressure gradient between them so that diffusivetransport is the only available mechanism of transport. Alternatively,water may be transferred across the membrane from the first fluid to thesecond fluid in some embodiments due to an induced pressure gradientbetween the fluids. The diffusive process may result in a filtered firstfluid that may be then transferred 625 from the filtration device.

An alternative embodiment for the method described by FIG. 6 is for anin vivo hemodialysis device including several membrane chipsmanufactured as described above. The device may also performhemofiltration or ultrafiltration. The filtration device may bedeveloped with a plurality of 1 cm square chips of the structurespreviously described. The chips may be oriented within the filtrationdevice to create channels as described previously, so that a first fluidcan be flowed between the channel formed by the front side of two chips,or across the membranes, and a second fluid can be flowed between thechannel formed by the backsides of two chips, or across the membranebackside through the cavity formed in the substrates. The two fluids maybe kept fluidly separate from each other by the chips such that transfercan only occur across the membranes. The formed filter may be housed ina biocompatible housing and implanted within a body. Connections may bemade internally to deliver blood to the filtration device through anarterial connection and return blood to a venous connection.Alternatively, a graft, fistula, cannula, or some other connection canbe used to reduce the number of internal connections. A second fluid maybe delivered to the filtration device from an external source, and maybe delivered to the device through the body via a port, catheter, orsome other device providing access internally. Once passed through thedevice, the second fluid may be returned via the same port or catheter,or through a secondary port or catheter. The second fluid may be flowedthrough the device in a continuous loop, or may be infused for a periodof time for use followed by a drainage process. Additional devicesincluding pumps may be similarly disposed within or out from the body,and may be incorporated directly with the filtration device. Similarlysensors may be disposed within or out of the device for monitoring anynumber of vital statistics along with additional numbers includingglucose level.

As described in FIG. 6, the first fluid, which may be blood, isdelivered 610 to the filtration device through the internal connectionsin the body. The first fluid is flowed 615 through the device over themembrane front side. The flowing 615 may additionally include a circuitthrough the device that passes the first fluid through a series ofchannels as described previously. Alternatively, the flow is dispersedacross a number of channels before being returned to a single outlet. Asecond fluid is flowed 620 across the backside of the membrane, and mayadditionally be flowed via a circuit through the device that passes thefirst fluid through a series of channels on the backside of themembranes. The second fluid may be dispersed across a number of channelsbefore being returned to a single outlet in a similar fashion to thefirst fluid. The first and second fluids may be kept fluidly separate bythe circuits such that transfer between the fluids may occur through themembranes. The first and second fluids may be pumped through thefiltration device in order to maintain equal pressure across themembrane section of the filtration device. The first fluid may flow 625or be pumped from the filtration device and return to the venous systemof the body.

FIG. 7 shows a graph of the diffusion resistance associated with afilter structure. An evaluation was performed to determine the relativeresistance through an exemplary filtration device. The evaluated deviceincluded six chips having lateral dimensions of 1 cm on a side. Eachchip had a 0.5 μm thick membrane over a 400 μm thick substrate. Asdisplayed to the left of the figure, the exemplary filter structurecomprises a membrane 715 over a substrate 705. As shown, a distance isrepresented as A to B for the distance from the bottom of the substrateto the bottom of the membrane structure. A distance is also representedas B to C for the distance from the bottom of the membrane structure tothe top of the membrane structure. Hence, a distance A to C shows thedistance through which diffusion may progress for an exemplaryfiltration device. The associated chart shows the concentration gradientfrom point A, as depicted by the left end of the X-axis, to point C, asdepicted by the right end of the X-axis. The inflection point 717represents point B, or the interface between the membrane and thesubstrate. As can be seen, only 5% of the concentration gradient occursbetween points B and C, or across the membrane. 95% of the concentrationgradient, and accordingly 95% of the transport resistance occurs throughthe substrate. The species diffusion resistance through a channel can bemodeled as a function of the length of the channel divided by theproduct of the diffusion coefficient for the species and thecross-sectional area for the channel. Hence, as the length increases, orthe area decreases, the resistance increases proportionately.Accordingly, by reducing the length of the diffusive channel, aproportionate decrease in the diffusive resistance can be expected. Putanother way, if the same level of resistance can be tolerated by thesystem, by reducing the length for diffusive transport, a reduced areamay be utilized to provide the same degree of function.

FIG. 8 shows a graph of the modeled flow of a fluid along the backsideof a filter fabricated according to embodiments of the presenttechnology. The fluid flows into a cavity formed in the backside of afiltration device, and delivers the fluid to diffusive recesses 830. Thediffusive recesses 830 along with porous membrane 815 allow diffusivetransport between the fluid and an additional fluid that may be flowedacross the top side of the membrane 815. By providing a cavity throughwhich the fluid may be delivered, the refresh rate of fluid transfer maybe improved near the diffusive recesses 830. Additionally, the diffusivetransport may be improved due to the reduced distance through whichdiffusion occurs, which may provide a concomitant reduction in thesystem transport resistance.

Turning to FIG. 9, cross-sectional views of exemplary filter structuresare shown according to embodiments of the present technology. Thefigures illustrate an additional process for performing the backsideetching of the filter structures. Some or all of the steps as previouslydescribed with respect to other structures may be incorporated into theprocesses as illustrated. FIG. 9A shows a portion of a filter structureafter front side processing has been performed. Substrate 905 mayinclude overlying protective oxide 910, as well as polymeric material915 including the defined pores. The materials may include any of thematerials as previously described with respect to other structures.Additionally, the pores in polymeric material 915 may include any of thestructures or dimensions as previously described. After front sideprocessing has been completed, the backside protective layer 920 may beformed and patterned as illustrated. Protective layer 920 may includeany of the materials as previously described and may include an oxidelayer similar to or different from layer 910. The patterning of backsidelayer 920 may be performed to define the recess areas through whichaccess to the filter membranes may be achieved as previously described,and may specifically define the cavity structures to be formed prior toor during the formation of the recess areas. The recesses may be of anyof the dimensions or geometries as previously described, and may be, forexample, about 10 mm×10 mm or less, and maybe for example 8 mm×8 mm, 6mm×6 mm, 4 mm×4 mm, 2 mm×2 mm, etc. or less.

After backside layer 920 has been patterned, an additional layer ofmaterial 925 may be formed over the backside structures. Material 925may be any of the previously described materials, and may be, forexample, a resist layer. Material layer 925 may be formed over andwithin the cavity areas defined by the patterning of backside layer 920,in order to define the recess or window layers for the final filters.Depending on the desired dimensioning of the windows, the positioning ofthe material layer 925 may be adjusted accordingly. The defined windowsmay be of any of the dimensions as previously described, and may be of avariety of geometries as may be useful in the final filters. Forexample, the windows may be defined as rectangles having a firstdimension longer than a second dimension. Either or both of the firstdimension and second dimension may be greater than or less than about500 μm in disclosed embodiments. Alternatively, either or both of thefirst dimension and second dimension may be less than or equal to about400 μm, 300 μm, 250 μm, 200 μm, 150 μm, 100 μm, 50 μm, 25 μm, 15 μm, 10μm, 5 μm, etc. or less. For example, the first dimension may be lessthan or about 300 μm, and the second dimension may be less than or about100 μm.

As illustrated in FIG. 9B, resist 925 may be deposited over thepatterned oxide layer 920, as well as within the defined recess regions.An etching process may be performed in order to etch through thebackside of substrate layer 905. The etching may be performed via any ofthe processes as previously described, and may be for example, a DRIEetch. The DRE etch may be performed to a depth in order to define thelength of the final support structure required between window sections.For example, the deeper the initial etch performed, the thicker thesupport structure remaining. The etch may be performed to a depthgreater than or less than about 5 μm, and may be performed greater thanor about 10 μm, 20 μm, 30 μm, 40 μm, 50 μm, 60 μm, 75 μm, 90 μm, 100 μm,125 μm, 150 μm, 200 μm, etc. or more. After the required etch depth hasbeen reached, the etch process may be stopped and material layer 925 maybe stripped. The exposed substrate 905 may include a stepped structurewithin the recess regions due to the material layer 925 preventingregions of the substrate 905 from being exposed to the etch process. Asecond etch process may be performed that is similar to or differentfrom the previous etch process. For example, a second DRIE etch may beperformed down to the layer of oxide 910. Because the etch process maybe uniform across the surface of the substrate 905, the steppedstructure may be maintained to the level of oxide layer 910.Accordingly, the steps originally protected by material layer 905 may bethe only remaining material upon the completion of the etch process.Final finishing may then be performed to remove the exposed regions ofoxide layer 910, which may then expose the filter regions that may befurther protected and supported by the remaining substrate sections 907.

Turning to FIG. 10, cross-sectional views of exemplary filter structuresare shown according to embodiments of the present technology. Thefigures illustrate an additional process for performing the backsideetching of the filter structures. Some or all of the steps as previouslydescribed with respect to other structures may be incorporated into theprocesses as illustrated. Substrate 1005 may include overlyingprotective oxide 1010, as well as polymeric material 1015 including thedefined pores. The materials may include any of the materials aspreviously described with respect to other structures. Additionally, thepores in polymeric material 1015 may include any of the structures ordimensions as previously described. After front side processing has beencompleted, the backside protective layer 1020 may be formed andpatterned as illustrated. Protective layer 1020 may include any of thematerials as previously described and may include an oxide layer similarto or different from layer 1010. Protective layer 1020 may be patternedto include both large and small openings as illustrated in FIG. 10A. Thesmall openings may include spacing between each section of material 1020of from less than or about 1 μm to about 100 μm or more in disclosedembodiments. The spacing may be less than, greater than, or about 5 μm,10 μm, 15 μm, 20 μm, 25 μm, 30 μm, 35 μm, 40 μm, 45 μm, 50 μm, 55 μm, 60μm, 65 μm, 70 μm, 75 μm, 80 μm, 85 μm, 90 μm, 95 μm, 100 μm, etc. ormore.

An etching process may be performed to remove the exposed regions ofsubstrate 1005. Oxide layer 1010 may be used as an etch stop for theetching process. Any of the previously described etching processes maybe performed, and a DRIE etch may be performed as previously described.The patterning of protective layer 1020 forming both large and smallopenings may be used to take advantage of a natural phenomenon known asaspect-ratio-dependent-etch rate, or ARDE. This phenomenon may causesmaller area recesses to etch more slowly than larger regions.Accordingly, when larger regions have been etched down to layer 1010,areas between the smaller openings in layer 1020, such as region 1007,may not be etched down to the layer of oxide layer 1010. The DRIE etchmay be an anisotropic etch, and may not suffer from edge creep into theregions under protective layer 1020. A subsequent isotropic etch may beperformed to undercut the remaining pillar structures around region1007, leaving support regions 1007 between the exposed filter sections.The isotropic etch may be any wet or dry etch as previously discussed,and may be, for example, an SF₆ preparation. The isotropic etch mayadditionally undercut support pillars 1008, as illustrated in FIG. 10C.Accordingly, in order to ensure adequate support structure around thecavities for each chip, this undercut may be compensated for in theinitial masking process. A benefit of such a process is that only onebackside mask may be needed, which may reduce queue times.

Turning to FIG. 11, cross-sectional views of exemplary filter structuresare shown according to embodiments of the present technology. Thefigures illustrate an additional process for performing the backsideetching of the filter structures. Some or all of the steps as previouslydescribed with respect to other structures may be incorporated into theprocesses as illustrated. Substrate 1105 may include overlyingprotective oxide 1110, as well as polymeric material 1115 including thedefined pores. The materials may include any of the materials aspreviously described with respect to other structures. Additionally, thepores in polymeric material 1115 may include any of the structures ordimensions as previously described. After front side processing has beencompleted, the backside protective layer 1120 may be formed andpatterned as illustrated. Protective layer 1120 may include any of thematerials as previously described and may include an oxide layer similarto or different from layer 1110. Protective layer 1120 may be patternedto include both large and small openings as illustrated in FIG. 11A,which may include any of the dimensions as previously discussed.Protective layer 1120 may be formed to compensate for expected removalthat may occur during the process. Layer 1120 may be, for example, a lowtemperature oxide formed to a thickness greater than or about 1 μm, andmay be greater than or about 2 μm, 5 μm, 7 μm, 10 μm, etc. or more. Thismaterial may have a known selectivity with respect to the substrate1105, such as a silicon substrate, based on the etch process beingperformed. For example, a low temperature oxide may have a selectivitycompared to silicon of about 100:1 for a certain etch process, such as aDRIE etch process.

An additional layer 1125 may be formed over the patterned protectivelayer 1120 as well as within the exposed recess regions. Larger andsmaller areas between portions of material 1125 may be formed asillustrated, for example. Layer 1125 may be any of the previouslydescribed layers, and may be, for example, a resist layer. An initialetch may be performed down to a first depth, which may be based on adesired thickness for the final support structures. The first etch maybe a substantially anisotropic etch and may be, for example, a DRIEetch. The first etch may be performed to a first depth through substrate1105, and the first depth may be greater than or about 1 μm, and may begreater than or about 2 μm, 5 μm, 10 μm, 15 μm, 20 μm, 25 μm, 30 μm, 50μm, etc. or more in disclosed embodiments. After the first depth hasbeen reached, the etching process may be stopped, and resist layer 1125may be stripped from the substrate and overlying protective layer 1120.The etching process may then be resumed down to the level of protectivelayer 1110, which may again act as an etch stop for the etching process.As explained previously with respect to other described processes, thestepped structure formed across the exposed recess regions of substrate1105 may be maintained throughout the etching process down to the levelof layer 1110. Depending on the etching process performed, the etch mayadditionally affect protective layer 1120, however based on theselectivity to the oxide as compared to silicon, for example, as well asthe initial amount of protective layer 1120 deposited, protective layer1120 may not be completely removed during the processing in order toprotect or maintain the cavity structure. As with the previous approach,this process may reduce the number and types of etchings that may beperformed, and may similarly reduce overall queue times during devicefabrication.

In an alternative embodiment, resist layer 1125 may be formed andpatterned with large and small divider areas prior to, or in lieu of,the formation of protective layer 1120. An initial etch may be performedover the resist layer 1125 as previously described down to a first depthwithin the substrate 1105. Etch layer 1125 may then be stripped. Anadditional resist layer may be formed over the support structuresbetween recess regions while leaving the stepped structure previouslyformed within the recess regions exposed. In disclosed embodiments, theadditional resist may not fully cover the support structures in order toallow for over-exposure of a subsequent etching process. The subsequentetch may then be capable of removing pooled resist that may remainwithin the formed cavities in the stepped structure of the substrate1105, for example. For example, UV exposure may be used to removeunwanted resist remaining within the stepped structure. As illustratedin FIG. 11C, an etching process such as a DRIE etch may then beperformed in order to remove the exposed stepped structure of thesubstrate 1105 down to the level of protective layer 1110. Any remainingresist may then be stripped from the final filter structure beforefinishing processes are performed. Such a process may be advantageousbecause an additional oxide layer may not be needed. Because such alayer may require additional or substantial time to form, removing sucha layer from the process may further improve queue times.

Turning to FIG. 12, cross-sectional views of exemplary filter structuresare shown according to embodiments of the present technology. Thefigures illustrate an additional process for performing the backsideetching of the filter structures. Some or all of the steps as previouslydescribed with respect to other structures may be incorporated into theprocesses as illustrated. Substrate 1205 may include overlyingprotective oxide 1210, as well as polymeric material 1215 including thedefined pores. The materials may include any of the materials aspreviously described with respect to other structures. Additionally, thepores in polymeric material 1215 may include any of the structures ordimensions as previously described. After front side processing has beencompleted, the backside protective layer 1220 may be formed andpatterned as illustrated. Protective layer 1220 may include any of thematerials as previously described and may include an oxide layer similarto or different from layer 1210. Protective layer 1220 may be patternedto provide a plurality of access regions through substrate 1205, whichmay have any of the dimensions as previously listed. Protective layer1220 may be of a variety of thicknesses as previously described, and maybe greater than or about 10 Å in disclosed embodiments, and mayadditionally be greater than or about 25 Å, 50 Å, 75 Å, 1 μm, 2 μm, 5μm, etc. or more. A resist layer 1225, or additional protective layer,may be formed over the edge supports in order to protect these regionsfrom subsequent etching processes. The resist layer 1225 may be of asimilar dimension to the corresponding portion of protective layer 1220over which it lies, and may be slightly smaller, for example, in orderto allow for removal of edge regions of the exposed recesses.

An etch process such as previously described, for example, may beperformed over the exposed structures. As illustrated in FIG. 12B, anetch process may be performed that etches both protective layer 1220 aswell as substrate 1205, although at different rates. For example,protective layer 1220 may be an oxide layer that etches slower than thematerial of substrate 1205, such as silicon, for example. The protectivelayer 1220 material, the thickness of the layer, as well as the etchprocess performed may all be adjusted in order to produce the desiredstructure. For example, protective layer 1220 may be formed of amaterial that has a known selectivity for a particular etch process ascompared to silicon. For example, the selected material may have aselectivity of greater than or about 50:1 as compared to silicon, or maybe greater than or about 75:1, 100:1, 120:1, 150:1, etc. or more. Thehigher the selectivity, the slower the material will etch as compared tosilicon, and the thicker remaining portions 1207 will be. The portionsof protective layer 1220 covering support sections 1207 may or may notbe completely etched during the process, which may or may not allowetching of underlying regions 1207. As illustrated in FIG. 12D, such aprocess may provide fairly uniform structures across a substrate and maycompensate for intra-wafer non-uniformity by adjusting the oxidethickness at different areas on the wafer. For example, oxide layer 1220may be formed thicker towards the edge regions of the areas to beremoved. Additionally, the process may not require deep-pit lithographyor re-patterning once the etch process is started, and therefore such afabrication process may be performed with a single etch down to thelayer of the filter membranes or underlying protective oxide layer 1210.Additionally, by utilizing a material with a higher selectivity ratio ascompared to silicon, less of the material may need to be deposited forthe process, which may further reduce queue times.

Turning to FIG. 13, cross-sectional views of exemplary filter structuresare shown according to embodiments of the present technology. Thefigures illustrate an additional process for performing themanufacturing of the filter structures. As will be understood, thefigures disclosed may illustrate only a portion of a larger filterstructure, such as illustrated in FIG. 2, for example. Some or all ofthe steps as previously described with respect to other structures maybe incorporated into the processes as illustrated. Protective layer1320, such as an oxide, may be formed and patterned over a substrate1305 in order to produce a stepped structure such as illustrated in FIG.13A. This protective layer 1320 may be formed over what will become thebackside of substrate 1305. The substrate 1305 may then be flipped andbonded to a subsequent wafer. Substrate 1305 may then be planarized to adesired thickness of the final filter supports, and front sideprocessing may be performed as previously described, which may includeforming protective layer 1310 and filter layer 1315 as illustrated.Planarizing substrate 1305 may reduce the thickness of the substrate1305 below about 1 mm, and may reduce the thickness of the substrate tobelow or about 750 μm, 500 μm, 250 μm, 100 μm, 75 μm, 50 μm, 25 μm, 15μm, 10 μm, 5 μm, etc. or less.

As illustrated in FIG. 13C, an etch may be performed through the bondedwafer to expose the stepped layer 1320. A subsequent etch or the sameetch through the bonded wafer may be performed through the protectivelayer 1320 and substrate 1305 down to the level of protective layer1310. The stepped structure of layer 1320 may allow supports 1307 to bemaintained based on similar selectivity principles as previouslydescribed, due to the thicker portions of layer 1320 overlying thoseregions. As illustrated in FIG. 13D, the thicker portions of layer 1320may or may not be completely etched during the process, and may maintaina portion of layer 1320 such as illustrated with sections 1322.

Turning to FIG. 14, cross-sectional views of exemplary filter structuresare shown according to embodiments of the present technology. Thefigures illustrate an additional process for performing the backsideetching of the filter structures. Some or all of the steps as previouslydescribed with respect to other structures may be incorporated into theprocesses as illustrated. Substrate 1405 may include overlyingprotective oxide 1410, as well as polymeric material 1415 including thedefined pores. The materials may include any of the materials aspreviously described with respect to other structures. Additionally, thepores in polymeric material 1415 may include any of the structures ordimensions as previously described. After front side processing has beencompleted, the backside protective layer 1420 may be formed over thesupport structure regions of substrate 1405. An etch producing slopedwalls within substrate 1405 may be performed, such as the KOH etch aspreviously described almost down to the protective layer 1410, such aswithin about 10 μm, 5 μm, 1 μm, 800 nm, 600 nm, 500 nm, 400 nm, 300 nm,250 nm, 200 nm, 150 nm, 100 nm, 50 nm, etc., or less. A resist layer1421 may be formed over the substrate structure, and as illustrated inFIG. 14B, may pool within the formed recess in the substrate 1405. Alithography process utilizing UV exposure may be performed with contactmask features 1424. Such a process may remove the exposed resist, whilemaintaining the portions residing under the defined contact maskregions. A subsequent etch may be performed through a portion of theexposed substrate 1405 prior to stripping remaining resist material 1421down to the layer of protective layer 1410. Such a process may providemore uniform intra-wafer depth control based on the wet etch performedinitially. Additionally, performing a wet etching process, such asdescribed throughout the specification may allow for batch processing ofmany wafers at a time, which may further reduce queue times.

Turning to FIG. 15, cross-sectional views of exemplary filter structuresare shown according to embodiments of the present technology. Thefigures illustrate an additional process for performing the backsideetching of the filter structures. Some or all of the steps as previouslydescribed with respect to other structures may be incorporated into theprocesses as illustrated. Substrate 1505 may include overlyingprotective oxide 1510, as well as polymeric material 1515 including thedefined pores. The materials may include any of the materials aspreviously described with respect to other structures. Additionally, thepores in polymeric material 1515 may include any of the structures ordimensions as previously described. After front side processing has beencompleted, the backside protective layer 1520 may be formed andpatterned as illustrated. Protective layer 1520 may include any of thematerials as previously described and may include an oxide layer similarto or different from layer 1510. Protective layer 1520 may be patternedto provide a plurality of gaps exposing regions of substrate 1505. Anetching process may be performed down to a first depth through thesubstrate 1505. The first depth may be based on the desired finalthickness of support structures that may be maintained between filterareas. For example, the first depth may be greater than or about 5 μm,and may be greater than or about 10 μm, 15 μm, 20 μm, 30 μm, 40 μm, 50μm, 60 μm, 75 μm, 100 μm, 150 μm, etc. or more. Such a process mayproduce a series of shallow trenches within the substrate 1505.

The backside protective layer 1520 may be removed from the substrate1505, and an anneal or subsequent process may be performed to merge theseries of shallow trenches into one or more cavities 1506 within thesurface of the substrate 1505. Depending on the number and patterning ofthe shallow trenches, cavities 1506 may form voids, pipes, plates, orother geometries within the substrate 1505. An additional material layer1523, such an oxide or resist, for example, may be deposited andpatterned over the regions of the substrate 1505 corresponding tosupport structures between final filter sections, such as the cavitiesas previously described. An etch process may then be performed throughthe exposed substrate. Because of the cavities 1506 within the substratestructure, regions of the substrate 1505 in line with the cavities 1506may etch at a faster rate than regions of the substrate 1505 stillintact. The etch process may be performed down to the level ofprotective layer 1510, and based on the cavities 1506 locations, supportstructures 1507 may be maintained between the window areas that mayexpose the filter regions. Turning to FIG. 16, SEM images are shown ofan annealing process used to convert a series of narrow trenches withina substrate into a void under the substrate surface as described above.

In the preceding description, for the purposes of explanation, numerousdetails have been set forth in order to provide an understanding ofvarious embodiments of the present technology. Having disclosed severalembodiments, it will be recognized by those of skill in the art thatvarious modifications, alternative constructions, and equivalents may beused without departing from the spirit of the disclosed embodiments.Additionally, a number of well-known processes and elements have notbeen described in order to avoid unnecessarily obscuring the presenttechnology. It will be apparent to one skilled in the art, however, thatcertain embodiments may be practiced without some of these details, orwith additional details. Accordingly, the above description should notbe taken as limiting the scope of the technology.

It is noted that individual embodiments may be described as a processthat is depicted as a flowchart, a flow diagram, or a block diagram.Although a flowchart may describe the method as a sequential process,many of the operations may be performed in parallel or concurrently. Inaddition, the order of the operations may be rearranged. A process maybe terminated when its operations are completed, but could haveadditional steps not discussed or included in a figure. Furthermore, notall operations in any particularly described process may occur in allembodiments. A process may correspond to a method, a function, aprocedure, a process, a subprocess, etc.

Where a range of values is provided, it is understood that eachintervening value, to the smallest fraction of the unit of the lowerlimit, unless the context clearly dictates otherwise, between the upperand lower limits of that range is also specifically disclosed. Eachsmaller range between any stated value or intervening value in a statedrange and any other stated or intervening value in that stated range isencompassed. The upper and lower limits of those smaller ranges mayindependently be included or excluded in the range, and each range whereeither, neither, or both limits are included in the smaller ranges isalso encompassed within the technology, subject to any specificallyexcluded limit in the stated range. Where the stated range includes oneor both of the limits, ranges excluding cither or both of those includedlimits are also included.

As used herein and in the appended claims, the singular forms “a”, “an”,and “the” include plural references unless the context clearly dictatesotherwise. Thus, for example, reference to “a dielectric material”includes a plurality of such materials, and reference to “the materiallayer” includes reference to one or more material layers and equivalentsthereof known to those skilled in the art, and so forth.

Also, the words “comprise”, “comprising”, “include”, “including”, and“includes”, “contains,” “containing,” etc., when used in thisspecification and in the following claims, are intended to specify thepresence of stated features, integers, components, or steps, but they donot preclude the presence or addition of one or more other features,integers, components, steps, acts, or groups.

1.-21. (canceled)
 22. A method of making a microfabricated filtrationdevice, the method comprising: depositing a dielectric layer over asemiconductor substrate; forming a first layer of a membrane material onthe dielectric layer and etching a pattern in the first membranematerial layer; forming a sacrificial dielectric layer over thepatterned first membrane material layer and forming a second membranematerial layer over the sacrificial dielectric layer; forming aprotective layer over the second membrane material layer; etching thesubstrate with a first etchant process that produces a cavity that doesnot extend to the layers of membrane material; etching the substratewith a second etchant process that forms a plurality of recesses throughthe remaining portion of the substrate and through the dielectric layer;and etching the filtration device with a third etchant process thatremoves the sacrificial dielectric layer forming pores through themembrane material layers, which provides access to the recesses suchthat the combination of the pores, recesses, and the cavity produceapertures through the filtration device.
 23. The method of claim 22,wherein the first etchant process comprises a wet etchant.
 24. Themethod of claim 23, wherein the first etchant process is anisotropic.25. The method of claim 23, wherein the first etchant process isisotropic.
 26. The method of claim 22, wherein the first and secondetchant processes comprise a reactive ion etch.
 27. The method of claim22, wherein the membrane material comprises silicon or polysiliconmembrane.
 28. The method of claim 27, wherein the pores have a width ofless than 100 nm.
 29. The method of claim 27, wherein the pores have awidth of less than 10 nm.
 30. The method of claim 28, wherein theplurality of recesses are rectangular and repeat along a width of thecavity and along a length of the cavity, the plurality of recesses eachcomprising a length of 500 μm or less.
 31. The method of claim 29,wherein the plurality of recesses comprise length by width measurementsof 100 μm by 50 μm.
 32. The method of claim 29, wherein the plurality ofrecesses comprise length by width measurements of 250 μm by 50 μm. 33.The method of claim 22, wherein the pores have a width of less than 100nm.
 34. The method of claim 22, wherein the pores have a width of lessthan 10 nm.
 35. The method of claim 22, wherein the plurality ofrecesses are rectangular and repeat along a width of the cavity andalong a length of the cavity, the plurality of recesses each comprisinga length of 500 μm or less.
 36. The method of claim 22, wherein theplurality of recesses comprise length by width measurements of 100 μm by50 μm.
 37. The method of claim 22, wherein the plurality of recessescomprise length by width measurements of 250 μm by 50 μm.
 38. The methodof claim 22, wherein the protective layer comprises silicon nitride,silicon oxide, silicon oxynitride, or silicon carbide.